CN105449166A - Manufacturing method for negative electrode pole piece for sodium ion battery - Google Patents

Manufacturing method for negative electrode pole piece for sodium ion battery Download PDF

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Publication number
CN105449166A
CN105449166A CN201510801013.3A CN201510801013A CN105449166A CN 105449166 A CN105449166 A CN 105449166A CN 201510801013 A CN201510801013 A CN 201510801013A CN 105449166 A CN105449166 A CN 105449166A
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Prior art keywords
sodium
ion battery
pole piece
active
cathode pole
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CN105449166B (en
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王开学
马超
李梅
陈接胜
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/60Selection of substances as active materials, active masses, active liquids of organic compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention relates to a manufacturing method for a negative electrode pole piece for a sodium ion battery. The manufacturing method comprises the steps of uniformly grinding an active material, and performing vacuum drying to obtain the active material used for the negative electrode of the sodium ion battery; performing slurry mixing from the active material, a conductive agent and a binder based on proportion, and uniformly coating a current collector copper foil with the slurry, and then performing vacuum drying and tabletting to obtain the negative electrode pole piece for the sodium ion battery. Compared with the prior art, the manufacturing method provided by the invention is simple. An electrochemical test proves that the negative electrode pole piece is high in cycling stability, and relatively high in specific discharge capacity; the first time discharge capacity can reach 568mAh/g under the current density of 100mA/g; after the battery is circulated for 50 times, the discharge capacity still can be stabilized at 194mAh/g; and meanwhile, the manufacturing method is high in economic benefit and applicable to large-scale production.

Description

A kind of manufacture method of sodium-ion battery cathode pole piece
Technical field
The invention belongs to sodium-ion battery technical field, especially relate to a kind of manufacture method of sodium-ion battery cathode pole piece.
Background technology
Along with day by day highlighting of energy crisis, greatly developing novel energy-storing system becomes one of study hotspot of researcher instantly.New forms of energy are as the pillar of novel industry, and the development of various novel energy-storing system electronics receives the concern of numerous industry.From portable electric appts, cell phone, notebook computer, arrive power vehicle etc., people also become large to the demand of secondary cell thereupon.Traditional secondary cell specific energy is lower, cannot meet the demand of people, and therefore, the energy-storage system developing novel high-energy-density of future generation seems particularly important.
In the last few years, lithium ion battery technology obtained vigorous growth, and a large amount of lithium ion battery devices is also widely used.But, in lithium ion battery, lower as indispensable elemental lithium reserves abundance on earth.Along with the extensive use of lithium ion battery, the demand of elemental lithium also increases year by year.Therefore, it is also proposed higher requirement to exploitation exploitation lithium, meanwhile, this also will play inhibitory action to a certain extent to large-scale production rechargeable lithium ion batteries energy storage device.Sodium element, belongs to same major element with elemental lithium in the periodic table of elements.The rich reserves of sodium element not only in the earth's crust, reserves are in the seawater also quite large.Be similar in electrochemical reaction medium power scholarship and moral conduct, therefore our chargeable sodium-ion battery that sodium element can be replaced elemental lithium mass production of cheap be easy to get.
(the XuehangWu such as WuXuehang, WenweiWun, KaituoWang, WenChenandDanHe. " Synthesisandelectrochemicalperformanceofflower-likeMnCo2 O4asananodematerialforsodiumionbatteries " MaterLett., 2015,147,85-87.) report a kind of negative material of cobalt acid manganese material as sodium-ion battery being similar to colored shape, under 50mA/g current density, after circulation is enclosed in discharge and recharge 40, specific discharge capacity remains on 244mAh/g.Although the electrical property that this negative material obtains has certain advantage, but metal oxide de-/embedding sodium ion time, there is huge change in the volume of active material, until active material configuration subsides, departs from collector, and causes the decay of chemical property because of convergent-divergent.
Prabakar, (the Prabakar such as S.J.Richard, S.J.Richard, Jeong, JaehyangandPyo, Myoungho. " Nanoporoushardcarbonanodesforimprovedelectrochemicalperf ormanceinsodiumionbatteries " ElectrochimicaActa, 2015, 161, 23-31.) report and utilize sucrose to prepare a kind of nano-pore hard carbon, and using the negative material of this carbon as sodium-ion battery, under the current density of 20mA/g, first discharge specific capacity is 251mAh/g, charge and discharge cycles is after 100 weeks, specific discharge capacity remains on 213mAh/g.But the preparation method of this active material is complicated, and technique is tediously long, is difficult to realize suitability for industrialized production.
Summary of the invention
Object of the present invention is exactly provide the manufacture method of the sodium-ion battery cathode pole piece that a kind of specific discharge capacity is higher, stable cycle performance, result are reproducible to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A manufacture method for sodium-ion battery cathode pole piece, adopts following steps:
(1) active material ground evenly and carry out vacuumize, obtaining the active material for sodium-ion battery negative pole;
(2) be evenly applied on copper foil of affluxion body after active material, conductive agent, binding agent being sized mixing in proportion, vacuumize, compressing tablet, prepare sodium-ion battery cathode pole piece.
Active material described in step (1) is selected from the one in class chelates such as ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, Ferric Sodium Edetate or ethylenediamine tetraacetic acid disodium magnesium salt, preferably, ethylenediamine tetra-acetic acid can be adopted.Grind uniform active material at 60-150 DEG C of vacuumize 6-10h.
Conductive agent described in step (2) is one or more in superconduction carbon black, electrically conductive graphite or Ketjen black; Binding agent is one or more in Kynoar, carboxymethyl cellulose or sodium alginate.The mass ratio of active material, conductive agent and binding agent is (4-8): (5-1): 1.Middle vacuumize temperature is 60-150 DEG C, and the time is 5-12h, and pressure is 1-6Pa.
Sodium-ion battery cathode pole piece making obtained is as test electrode, and sodium metal, as to electrode, is assembled into CR2016 type button cell, and its septation is for commonly using glass fibre membrane in this field, and electrolyte is: 1MNaClO 4/ EC:DEC (1:1)+5wt%FEC, test charging and discharging currents density is 100mA/g.
Compared with prior art, the present invention is using class chelates such as ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, Ferric Sodium Edetate, ethylenediamine tetraacetic acid disodium magnesium salts as sodium-ion battery negative pole active material.Above-mentioned substance is of many uses, cheap and easy to get.In charge and discharge process, sodium ion can be free to replace H or metal ions M on the COOH of this kind of chelate (M) group, and realize embedding freely and deviating from, as the negative active core-shell material of sodium-ion battery, economic benefit is given prominence to, and under the current density of 100mA/g, first discharge specific capacity is 568mAh/g, after 50 circulations, specific discharge capacity still remains on more than 194mAh/g, has good electrochemical cycle stability.The invention provides a kind of active material and the cathode pole piece preparation that can be used for sodium-ion battery negative pole, method is simple, is easy to operation, and technological process is succinct, is applicable to large-scale production.
Accompanying drawing explanation
The SEM figure of the sodium-ion battery cathode pole piece of Fig. 1 prepared by embodiment 1;
Fig. 2 is the isothermal nitrogen adsorption desorption curve chart of the sodium-ion battery negative pole active material that embodiment 2 uses;
Fig. 3 is that sodium-ion battery cathode pole piece prepared by embodiment 2 is assembled into the first charge-discharge curve chart of battery;
Fig. 4 is that sodium-ion battery cathode pole piece prepared by embodiment 2 is assembled into the recycle ratio Capacity Plan of battery;
Fig. 5 is that sodium-ion battery cathode pole piece prepared by embodiment 3 is assembled into the recycle ratio Capacity Plan of battery.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Active material ethylenediamine tetra-acetic acid is positioned in vacuum drying chamber, after 60 DEG C of dry 10h, as sodium-ion battery negative active core-shell material.By this negative material, conductive agent superconduction carbon black (SP), binding agent Kynoar (PVDF) in mass ratio 6:3:1 mix, with 1-METHYLPYRROLIDONE (NMP) for solvent, evenly be applied on copper foil of affluxion body after sizing mixing, be positioned over vacuum drying chamber, at 60 DEG C after dry 12h, adopt 3Pa pressure compressing tablet, obtain sodium-ion battery cathode pole piece, Fig. 1 is the SEM figure of sodium-ion battery cathode pole piece.As can be seen from the figure, the surface ratio of electrode slice is comparatively even, can be found out by partial enlarged drawing, and it is relatively more even that active material disperses, and particle diameter is approximately between 50-100nm.
Embodiment 2
Active material disodium ethylene diamine tetraacetate is positioned in vacuum drying chamber, after 150 DEG C of dry 6h, as sodium-ion battery negative active core-shell material.By this negative material, electrically conductive graphite, binding agent sodium alginate (SA) in mass ratio 8:1:1 mix, take distilled water as solvent, evenly be applied on copper foil of affluxion body after sizing mixing, be positioned over vacuum drying chamber, at 150 DEG C after dry 5h, adopt 4Pa pressure compressing tablet, obtain sodium-ion battery cathode pole piece, Fig. 2,3,4 is respectively the isothermal nitrogen adsorption desorption curve chart of sodium-ion battery negative pole active material, sodium-ion battery cathode pole piece is assembled into battery first charge-discharge curve chart and recycle ratio Capacity Plan.As can be seen from the isothermal nitrogen adsorption desorption curve of Fig. 2 active material disodium ethylene diamine tetraacetate, middle nip territory (0.3-0.9), there is an obvious hysteresis loop in curve, illustrates that this kind of material has certain meso-hole structure; Higher-pressure region (0.9-1.0) adsorption curve has an obvious nose-up tendency, and adsorbance increases suddenly, shows to there is a large amount of fissure holes in this material.The existence of hole, can better wetting activity material, simultaneously also for the transmission of sodium ion provides a large amount of passages.Fig. 3 is the first charge-discharge curve chart of this cathode pole piece assembling sodium-ion battery, and first discharge specific capacity reaches 464mAh/g, and electric discharge occurs that the some position that turnover is is respectively about 1.0V and 0.75V.Fig. 4 is the charge and discharge cycles figure of battery.Under charging and discharging currents density is 100mA/g, battery is after electrochemical activation process, the specific discharge capacity of the 2nd week decays to 169mAh/g, in ensuing circulation, this battery shows good cyclical stability, after 50th week charge and discharge cycles, specific discharge capacity is still higher remains on 155mAh/g and efficiency for charge-discharge (=specific discharge capacity/charge specific capacity × 100%) remains on about 100% substantially.
Embodiment 3
Active material tetrasodium ethylenediamine tetraacetate is positioned in vacuum drying chamber, after 80 DEG C of dry 9h, as sodium-ion battery negative active core-shell material.By this negative material, Ketjen black, binding agent carboxymethyl cellulose (CMC) in mass ratio 7:2:1 mix, take distilled water as solvent, evenly be applied on copper foil of affluxion body after sizing mixing, be positioned over vacuum drying chamber, at 80 DEG C after dry 10h, adopt 2Pa pressure compressing tablet, obtain sodium-ion battery cathode pole piece, be assembled into battery, the recycle ratio capacity of this battery as shown in Figure 5.Fig. 5 is the charge and discharge cycles figure of battery.Under charging and discharging currents density is 100mA/g, first discharge specific capacity is up to 568mAh/g, after the electrochemical activation process of a week, the specific discharge capacity of the 2nd week reduces to 206mAh/g, in ensuing circulation, this battery shows good cyclical stability, and after the 50th week charge and discharge cycles, specific discharge capacity is still higher remains on 194mAh/g and efficiency for charge-discharge remains on about 100% substantially.
Embodiment 4
Active material Ferric Sodium Edetate is positioned in vacuum drying chamber, after 120 DEG C of dry 7h, as sodium-ion battery negative active core-shell material.By this negative material, conductive agent superconduction carbon black (SP), binding agent Kynoar (PVDF) in mass ratio 4:5:1 mix, with 1-METHYLPYRROLIDONE (NMP) for solvent, evenly be applied on copper foil of affluxion body after sizing mixing, be positioned over vacuum drying chamber, at 120 DEG C after dry 8h, adopt 1Pa pressure compressing tablet, obtain sodium-ion battery cathode pole piece.
Embodiment 5
Active material ethylenediamine tetraacetic acid disodium magnesium salt is positioned in vacuum drying chamber, after 100 DEG C of dry 8h, as sodium-ion battery negative active core-shell material.By this negative material, conductive agent superconduction carbon black (SP), binding agent sodium alginate (SA) in mass ratio 5:4:1 mix, take distilled water as solvent, evenly be applied on copper foil of affluxion body after sizing mixing, be positioned over vacuum drying chamber, at 70 DEG C after dry 11h, adopt 6Pa pressure compressing tablet, obtain sodium-ion battery cathode pole piece.
This experiment is assembled into CR2016 type button cell respectively to embodiment 1-5 gained sodium-ion battery cathode pole piece.This button cell is gained in each embodiment by cathode pole piece, is formed electrode metal sodium, fibreglass diaphragm, electrolyte and shell.Wherein electrolyte is: 1MNaClO 4/ EC:DEC (1:1 volume ratio, EC: ethylene carbonate, DEC: diethyl carbonate)+5wt%FEC (FEC: fluorinated ethylene carbonate).
LAND test macro is adopted under room temperature environment, to carry out electric performance test to the battery prepared by embodiment 1-5 gained sodium-ion battery negative pole respectively.Wherein, before testing sodium-ion battery is positioned in the environment of 40 DEG C and leaves standstill 2h; During test, charging and discharging currents density is 100mA/g, and discharge and recharge cut-ff voltage is 0.01-3V (vs.Na/Na +).

Claims (8)

1. a manufacture method for sodium-ion battery cathode pole piece, is characterized in that, the method adopts following steps:
(1) active material ground evenly and carry out vacuumize, obtaining the active material for sodium-ion battery negative pole;
(2) be evenly applied on copper foil of affluxion body after active material, conductive agent, binding agent being sized mixing in proportion, vacuumize, compressing tablet, prepare sodium-ion battery cathode pole piece.
2. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, it is characterized in that, the active material described in step (1) is selected from one or more of ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, Ferric Sodium Edetate or ethylenediamine tetraacetic acid disodium magnesium salt.
3. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, is characterized in that, the preferred ethylenediamine tetra-acetic acid of active material described in step (1).
4. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, is characterized in that, in step (1), the uniform active material of grinding is at 60-150 DEG C of vacuumize 6-10h.
5. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, is characterized in that, the conductive agent described in step (2) is one or more in superconduction carbon black, electrically conductive graphite or Ketjen black.
6. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, is characterized in that, the binding agent described in step (2) is one or more in Kynoar, carboxymethyl cellulose or sodium alginate.
7. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1 or 5 or 6, is characterized in that, in step (2), the mass ratio of active material, conductive agent and binding agent is (4-8): (5-1): 1.
8. the manufacture method of a kind of sodium-ion battery cathode pole piece according to claim 1, is characterized in that, in step (2), vacuumize pressure is 1-6Pa, and temperature is 60-150 DEG C, and the time is 5-12h.
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Cited By (5)

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CN106099064A (en) * 2016-08-03 2016-11-09 常州大学 A kind of SnS2the preparation method of/CNTs composite nano materials and the application as anode material of lithium-ion battery thereof
CN106848242A (en) * 2017-02-27 2017-06-13 苏州大学 A kind of organic lithium storage materials of high power capacity and its application
CN108172786A (en) * 2017-12-22 2018-06-15 上海交通大学 A kind of lithium cell cathode material based on fused ring compound and preparation method thereof
CN108269990A (en) * 2018-03-06 2018-07-10 广东工业大学 A kind of anode material of lithium-ion battery and preparation method thereof and battery
CN109565037A (en) * 2016-07-18 2019-04-02 宁德时代新能源科技股份有限公司 Sodium-ion battery pole piece, preparation method and the sodium-ion battery containing the pole piece

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109565037A (en) * 2016-07-18 2019-04-02 宁德时代新能源科技股份有限公司 Sodium-ion battery pole piece, preparation method and the sodium-ion battery containing the pole piece
CN106099064A (en) * 2016-08-03 2016-11-09 常州大学 A kind of SnS2the preparation method of/CNTs composite nano materials and the application as anode material of lithium-ion battery thereof
CN106099064B (en) * 2016-08-03 2019-12-06 常州大学 Preparation method of SnS2/CNTs composite nano material and application of composite nano material as negative electrode material of sodium-ion battery
CN106848242A (en) * 2017-02-27 2017-06-13 苏州大学 A kind of organic lithium storage materials of high power capacity and its application
CN108172786A (en) * 2017-12-22 2018-06-15 上海交通大学 A kind of lithium cell cathode material based on fused ring compound and preparation method thereof
CN108172786B (en) * 2017-12-22 2020-04-03 上海交通大学 Lithium battery negative electrode material based on condensed ring compound and preparation method thereof
CN108269990A (en) * 2018-03-06 2018-07-10 广东工业大学 A kind of anode material of lithium-ion battery and preparation method thereof and battery

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